Acetic Acid → 2-Propenoic acid, 3-phenyl-

HRID 617004ノート

反応式

HRID 617004 の反応式
C1(N(C2C=CC=CC=2)[C:8]([CH:10]=[CH:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[O:9])C=CC=CC=1.C(O)(=[O:26])C.S(=O)(=O)(O)O>O>[CH:10]([C:8]([OH:9])=[O:26])=[CH:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 1118Sulfuric AcidHCID 2769635N,N-Diphenylcinnamamide

生成物 1

HCID 87842-Propenoic acid, 3-phenyl-

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

The N,N-diphenylstyrenyl carboxamide-2% divinylbenzene copolymer from example 7(a) (53.0g) was heated with stirring at 130°-135° for 44 hours with a mixture of glacial acetic acid (670 ml.), concentrated sulphuric acid (500 ml.) and water (300 ml.). After cooling to room temperature, the mixture was filtered and the polymer washed successively with water (4 × 400 ml.), acetone (3 × 200 ml.); methanol (3 × 200ml.), water (2 × 400 ml.) and acetone (2 × 200 ml.); and dried in vacuo at 40° to constant weight. The title polymer (36.58g) was green in colour and exhibited ν max (NuJol) 1690 (C=O) and 3700-2400 (OH) cm-1. Titration was effected by suspending the product (0.500g) in 95% ethanol (50 ml.) adding 0.5M sodium hydroxide (50 ml.), warming the mixture to reflux, cooling and back titrating with 0.5M hydrochloric acid using phenolphthalein as the indicator; it was found that 47.12 ml. of acid were required for neutralisation indicating 2.88 m.mole carboxyl/g of polymer.

後処理

  1. filtrationthe mixture was filtered
  2. washthe polymer washed successively with water (4 × 400 ml.), acetone (3 × 200 ml.)
  3. customand dried in vacuo at 40° to constant weight
  4. additionadding 0.5M sodium hydroxide (50 ml.)
  5. temperaturewarming the mixture
  6. temperatureto reflux
  7. temperaturecooling

出典と根拠

ORDレコード
ord-24fb597460b64e418f2601c5614a6296
出典データセット
uspto-grants-1978_02
特許番号
US04076913

反応ノート

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